Substrate phosphorus segregation repair method for producing OLED metal mask plates

Abstract

The present invention provides a method for repairing phosphorus segregation of a substrate for producing an OLED metal mask plate, and relates to the technical field of metal mask plates. The present invention provides a method for repairing phosphorus segregation of a substrate for producing an OLED metal mask plate, comprising the following steps: performing low-tension high-temperature annealing treatment on an alloy raw material, applying low tension to the alloy raw material, and preheating, heating, and heat preservation and cooling the alloy raw material under the premise of maintaining low tension; performing high-tension low-temperature annealing treatment on the alloy raw material after the low-tension high-temperature annealing treatment, applying high tension to the alloy raw material, and preheating, heating, and heat preservation and cooling the alloy raw material under the premise of maintaining high tension. The technical effect of alleviating phosphorus segregation is achieved.

Description

Technical Field

[0001] The invention relates to the technical field of metal mask plates, and in particular to a method for repairing phosphorus segregation of a substrate used for producing an OLED metal mask plate. Background Art

[0002] Fine metal masks (FMMs) are crucial to the manufacture of OLED panels and are highly dependent on the low thermal expansion properties of Invar alloy to ensure the extraordinary display effect and long-term stability of display devices. However, during the production process of Invar alloy, especially during the smelting stage, if there are defects in the dephosphorization process, impurity element phosphorus may remain. The non-uniform distribution of phosphorus may cause defects in the microstructure of the alloy, which may be further exacerbated during the cold rolling process, posing a challenge to the precision and reliability of FMM manufacturing.

[0003] The cold rolling process is a key step in FMM manufacturing. It not only determines the thickness, surface gloss and roughness of the material, but also has a profound impact on the stress distribution and microstructure inside the material. During the cold rolling process, phosphorus segregation may lead to local stress concentration, increase the brittleness of the material, and may even induce cracks. These factors directly threaten the dimensional stability and morphological accuracy of FMM, and thus affect the accuracy of the entire manufacturing process and the performance of the final product.

[0004] More seriously, phosphorus segregation may cause uneven opening sizes during the etching process of Invar alloy, resulting in defects in the microporous structure of FMM. These defects will lead to uneven deposition of luminescent materials during the evaporation process of OLED panels, causing inconsistent local luminous intensity, affecting the brightness uniformity and color accuracy of the display, and ultimately damaging the overall display performance of the OLED panel. Summary of the invention

[0005] The object of the present invention is to provide a method for repairing phosphorus segregation of a substrate used for producing an OLED metal mask plate, so as to alleviate the technical problem of phosphorus segregation in the prior art.

[0006] In a first aspect, an embodiment of the present invention provides a method for repairing phosphorus segregation of a substrate for producing an OLED metal mask, comprising the following steps:

[0007] Perform low-tension high-temperature annealing treatment on the alloy raw materials, apply low tension to the alloy raw materials, and preheat, heat, keep warm and cool the alloy raw materials under the premise of maintaining low tension;

[0008] Among them, the low tension is set between 80-120N, the preheating time is set between 80-100 seconds, the preheating temperature is set between 280-320℃, the heating temperature is set between 880-950℃, the heating time is set between 580-650 seconds, the holding time is set between 750-850 seconds, and the alloy raw material is cooled to between 20-30℃ between 95-110 seconds;

[0009] After the low-tension high-temperature annealing treatment, the alloy raw material is subjected to a high-tension low-temperature annealing treatment, and high tension is applied to the alloy raw material, so that the alloy raw material is preheated, heated, kept warm and cooled while maintaining high tension;

[0010] Among them, the high tension is set between 180-220N, the preheating time is set between 80-100 seconds, the preheating temperature is set between 180-220℃, the heating temperature is set between 480-550℃, the heating time is set between 580-650 seconds, the insulation time is set between 450-550 seconds, and the alloy raw material is cooled to between 20-30℃ between 95-110 seconds.

[0011] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein in the low tension high temperature annealing stage, the low tension is set to 100N.

[0012] In combination with the first aspect, the embodiment of the present invention provides a possible implementation of the first aspect, wherein the preheating time is set to 90 seconds and the preheating temperature is set to 300° C.

[0013] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein the heating temperature is set to 900° C., the heating time is set to 600 seconds, and the insulation time is set to 800 seconds.

[0014] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein, in the low-tension high-temperature annealing cooling stage, the furnace temperature is set to 25° C., and inert gas is used for rapid cooling within 100 seconds.

[0015] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein in the high-tension low-temperature annealing stage, the high tension is set to 200N.

[0016] In combination with the first aspect, the embodiment of the present invention provides a possible implementation of the first aspect, wherein the preheating time is set to 90 seconds and the preheating temperature is set to 200°C.

[0017] In combination with the first aspect, the embodiment of the present invention provides a possible implementation of the first aspect, wherein the heating temperature is set to 500° C. and the heating time is set to 600 seconds.

[0018] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein the insulation time is set to 500 seconds.

[0019] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein, in the high-tension low-temperature annealing cooling stage, the furnace temperature is set to 25°C, and inert gas is used for rapid cooling within 100 seconds.

[0020] Beneficial effects:

[0021] The present invention provides a method for repairing phosphorus segregation of a substrate for producing an OLED metal mask plate, comprising the following steps: performing a low-tension high-temperature annealing treatment on an alloy raw material, applying low tension to the alloy raw material, and preheating, heating, heat preservation, and cooling the alloy raw material under the premise of maintaining low tension; wherein the low tension is set between 80-120N, the preheating time is set between 80-100 seconds, the preheating temperature is set between 280-320°C, the heating temperature is set between 880-950°C, the heating time is set between 580-650 seconds, the heat preservation time is set between 750-850 seconds, and the alloy is preheated between 95-110 seconds. The gold raw material is cooled to between 20-30°C; after the low-tension high-temperature annealing treatment, the alloy raw material is subjected to high-tension low-temperature annealing treatment, and high tension is applied to the alloy raw material, so that the alloy raw material is preheated, heated, kept warm and cooled under the premise of maintaining high tension; wherein, the high tension is set between 180-220N, the preheating time is set between 80-100 seconds, the preheating temperature is set between 180-220°C, the heating temperature is set between 480-550°C, the heating time is set between 580-650 seconds, the keeping time is set between 450-550 seconds, and the alloy raw material is cooled to between 20-30°C between 95-110 seconds.

[0022] Specifically, the Invar alloy treated by the substrate phosphorus segregation repair method used to produce OLED metal mask plates can not only significantly improve the phosphorus segregation problem, but also improve the microstructure and macro performance of FMM products, ensuring high precision and high reliability in the OLED panel manufacturing process. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0024] Figure 1This is the macroscopic image of the unannealed Invar alloy;

[0025] Figure 2 This is the microscopic image of Invar alloy without annealing treatment;

[0026] Figure 3 A macroscopic image of Invar alloy treated by the phosphorus segregation repair method for a substrate used for producing an OLED metal mask provided by an embodiment of the present invention;

[0027] Figure 4 A microscopic image of Invar alloy treated by the phosphorus segregation repair method for a substrate used for producing an OLED metal mask provided in an embodiment of the present invention. DETAILED DESCRIPTION

[0028] The technical solution of the present invention will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0029] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0030] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0031] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0032] The present invention is further described in detail below through specific embodiments in conjunction with the accompanying drawings.

[0033] The present embodiment provides a method for repairing phosphorus segregation of a substrate for producing an OLED metal mask plate, comprising the following steps: performing a low-tension high-temperature annealing treatment on an alloy raw material, applying low tension to the alloy raw material, and preheating-heating-insulating and cooling the alloy raw material under the premise of maintaining low tension; wherein the low tension is set between 80-120N, the preheating time is set between 80-100 seconds, the preheating temperature is set between 280-320°C, the heating temperature is set between 880-950°C, the heating time is set between 580-650 seconds, the insulation time is set between 750-850 seconds, and the insulation time is set between 95-110 seconds. The alloy raw material is cooled to between 20-30°C; after the low-tension high-temperature annealing treatment, the alloy raw material is subjected to high-tension low-temperature annealing treatment, and high tension is applied to the alloy raw material, so that the alloy raw material is preheated, heated, kept warm and cooled under the premise of maintaining high tension; wherein the high tension is set between 180-220N, the preheating time is set between 80-100 seconds, the preheating temperature is set between 180-220°C, the heating temperature is set between 480-550°C, the heating time is set between 580-650 seconds, the keeping time is set between 450-550 seconds, and the alloy raw material is cooled to between 20-30°C between 95-110 seconds.

[0034] Specifically, the Invar alloy treated by the substrate phosphorus segregation repair method used to produce OLED metal mask plates can not only significantly improve the phosphorus segregation problem, but also improve the microstructure and macroscopic performance of FMM products, ensuring high precision and high reliability in the OLED panel manufacturing process.

[0035] In an optional solution of this embodiment, during the low-tension high-temperature annealing stage, the low tension is set to 100N.

[0036] Among them, the preheating time is set to 90 seconds and the preheating temperature is set to 300°C.

[0037] Among them, the heating temperature is set to 900°C, the heating time is set to 600 seconds, and the insulation time is set to 800 seconds.

[0038] Among them, in the low-tension high-temperature annealing cooling stage, the furnace temperature is set to 25°C, combined with inert gas for rapid cooling within 100 seconds.

[0039] Specifically, in the low-tension high-temperature annealing stage, a low tension of 100N is applied to the Invar alloy raw material to reduce the stress level of the material, and then the Invar alloy raw material is gradually preheated to 300°C within 90 seconds. This step effectively reduces thermal stress and material deformation, laying the foundation for deep heat treatment, and then the material is further heated to 900°C for 600 seconds, using high temperature to promote the free diffusion of phosphorus in the lattice, effectively reducing phosphorus segregation, and maintained at 900°C for 800 seconds. The low tension and high temperature work together to promote the uniform distribution of phosphorus and grain recrystallization, further alleviating the segregation phenomenon. Finally, the furnace temperature is set to 25°C and combined with nitrogen inert gas for rapid cooling, so that the surface temperature of the Invar alloy raw material drops sharply within 100 seconds to release thermal stress, while fixing the grain structure, preparing for secondary high-tension low-temperature annealing.

[0040] It should be pointed out that the effects of low tension at high temperature include that low tension helps to reduce the internal stress caused by cold rolling inside the Invar alloy raw material; low tension reduces the resistance to atomic movement, making it easier for impurity elements such as phosphorus to diffuse in the lattice, thereby helping to reduce segregation; low tension helps the movement and rearrangement of dislocations, reducing dislocation accumulation, thereby reducing internal defects in the material.

[0041] It should also be pointed out that the low tension can also be set to 80N, or the low tension can also be set to 100N, or the low tension can also be set to 120N.

[0042] The preheating time can also be set to 80 seconds, and the preheating temperature can also be set to 320°C, or the preheating time can also be set to 90 seconds, and the preheating temperature can also be set to 300°C, or the preheating time can also be set to 100 seconds, and the preheating temperature can also be set to 280°C.

[0043] The heating temperature can also be set to 880°C, the heating time can also be set to 650 seconds, and the insulation time can also be set to 850 seconds. Alternatively, the heating temperature can also be set to 900°C, the heating time can also be set to 600 seconds, and the insulation time can also be set to 800 seconds. Alternatively, the heating temperature can also be set to 950°C, the heating time can also be set to 580 seconds, and the insulation time can also be set to 750 seconds.

[0044] The alloy feedstock may be cooled to 30° C. in 95 seconds, or to 25° C. in 100 seconds, or to 20° C. in 110 seconds.

[0045] In an optional solution of this embodiment, in the high-tension and low-temperature annealing stage, the high tension is set to 200N.

[0046] Among them, the preheating time is set to 90 seconds and the preheating temperature is set to 200°C.

[0047] The heating temperature was set to 500° C., and the heating time was set to 600 seconds.

[0048] Among them, the insulation time is set to 500 seconds.

[0049] Among them, in the high-tension low-temperature annealing cooling stage, the furnace temperature is set to 25°C, combined with inert gas for rapid cooling within 100 seconds.

[0050] Specifically, in the high-tension and low-temperature annealing stage, a low tension of 200N is applied to the Invar alloy raw material to promote a more uniform distribution of phosphorus in the lattice and reduce grain boundary segregation. Then the Invar alloy raw material is gradually heated to 200°C within 90 seconds to prevent band breakage under high tension. Then the material is further heated to 500°C and continuously heated for 600 seconds to create ideal temperature conditions for grain refinement under high tension, and maintained at 500°C for 500 seconds. High tension helps to further refine the grains, optimize the microstructure, and improve the overall uniformity of the material. Finally, the furnace temperature is set to 25°C and combined with nitrogen inert gas for rapid cooling, so that the surface temperature of the Invar material is sharply reduced within 100 seconds, the internal stress caused by heat treatment is reduced, and the stability of the microstructure is ensured.

[0051] It should be pointed out that in the high-tension and low-temperature annealing stage, the effects of high tension include that high tension helps to refine the grains during the low-temperature annealing process, reduce the number of grain boundaries, and reduce the possibility of phosphorus aggregation at the grain boundaries; high tension can reduce the tendency of phosphorus to segregate at the grain boundaries by changing the energy state of the grain boundaries.

[0052] It should also be pointed out that the low tension can also be set to 180N, or the low tension can also be set to 200N, or the low tension can also be set to 220N.

[0053] The preheating time can also be set to 80 seconds, and the preheating temperature can also be set to 220°C, or the preheating time can also be set to 90 seconds, and the preheating temperature can also be set to 200°C, or the preheating time can also be set to 100 seconds, and the preheating temperature can also be set to 180°C.

[0054] The heating temperature can also be set to 480°C, the heating time can also be set to 650 seconds, and the insulation time can also be set to 550 seconds. Alternatively, the heating temperature can also be set to 500°C, the heating time can also be set to 600 seconds, and the insulation time can also be set to 500 seconds. Alternatively, the heating temperature can also be set to 550°C, the heating time can also be set to 580 seconds, and the insulation time can also be set to 450 seconds.

[0055] The alloy feedstock may be cooled to 30° C. in 95 seconds, or to 25° C. in 100 seconds, or to 20° C. in 110 seconds.

[0056] As shown in Table 1 below, the embodiment and reference examples both selected mother rolls with phosphorus segregation phenomenon for conventional annealing treatment (one annealing, temperature 550 degrees, tension 10N) and restorative annealing treatment, and the treatment length was 300 meters. The comparative example selected mother rolls with phosphorus segregation phenomenon.

[0057] The samples of Example 1, Example 2 and Example 3 respectively correspond to the front, middle and back sections of the annealed coil treated by the improved substrate phosphorus segregation repair method for producing OLED metal mask plates of this embodiment to ensure the consistency of the treatment effect of the entire coil.

[0058] The samples of Reference Examples 1, 2 and 3 correspond to the front, middle and back stages of conventional annealing, respectively, to ensure the consistency of the treatment effect of the entire coil.

[0059] The samples of Comparative Examples 1, 2 and 3 correspond to the front, middle and back sections without annealing, respectively, to ensure the consistency of the treatment effect of the entire coil.

[0060] The surface of all samples was carefully observed using a standardized inspection method, recording the number of phosphorus segregation defects to evaluate the effect of the annealing process.

[0061]

[0062] Table 1

[0063] As shown in Table 1 above, the number of phosphorus segregation defects on the AB surface of Comparative Example 1, Comparative Example 2, and Comparative Example 3 (before annealing) are 22 / 27, 18 / 16, and 25 / 28, respectively, and the amount of phosphorus segregation defects does not decrease after thinning.

[0064] The numbers of phosphorus segregation defects on the AB planes in Reference Example 1, Reference Example 2 and Reference Example 3 (conventional annealing) were 15 / 13, 13 / 17 and 16 / 12, respectively, and the number of phosphorus segregation defects did not decrease after thinning.

[0065] The number of phosphorus segregation defects in Example 1, Example 2, and Example 3 (using a method for repairing phosphorus segregation of a substrate for producing an OLED metal mask) was 0, and no phosphorus segregation defects were detected after thinning.

[0066] See also Figure 1 and Figure 2 As shown, Figure 1 This is the macro image of the unannealed Invar alloy. Figure 2 This is a microscopic image of the Invar alloy without annealing treatment. Phosphorus segregation defects lead to defect points on the Invar alloy, which increases the brittleness of the Invar alloy and may even induce cracks. These factors directly threaten the dimensional stability and morphological accuracy of the FMM, and thus affect the accuracy of the entire manufacturing process and the performance of the final product.

[0067] See also Figure 3 and Figure 4 As shown, Figure 3 This is a macroscopic image of Invar alloy treated by the phosphorus segregation repair method for substrates used to produce OLED metal mask plates provided in this embodiment. Figure 4 This is a microscopic image of the Invar alloy treated by the phosphorus segregation repair method for a substrate used to produce an OLED metal mask provided in this embodiment. The surface of the Invar alloy treated by the phosphorus segregation repair method for a substrate used to produce an OLED metal mask provided in this embodiment is smooth and free of phosphorus segregation defects.

[0068] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for repairing phosphorus segregation of a substrate for producing an OLED metal mask, characterized in that: The following steps are involved: Perform low-tension high-temperature annealing treatment on the alloy raw materials, apply low tension to the alloy raw materials, and preheat, heat, keep warm and cool the alloy raw materials under the premise of maintaining low tension; Among them, the low tension is set between 80-120N, the preheating time is set between 80-100 seconds, the preheating temperature is set between 280-320℃, the heating temperature is set between 880-950℃, the heating time is set between 580-650 seconds, the holding time is set between 750-850 seconds, and the alloy raw material is cooled to between 20-30℃ between 95-110 seconds; After the low-tension high-temperature annealing treatment, the alloy raw material is subjected to a high-tension low-temperature annealing treatment, and high tension is applied to the alloy raw material, so that the alloy raw material is preheated, heated, kept warm and cooled while maintaining high tension; Among them, the high tension is set between 180-220N, the preheating time is set between 80-100 seconds, the preheating temperature is set between 180-220℃, the heating temperature is set between 480-550℃, the heating time is set between 580-650 seconds, the insulation time is set between 450-550 seconds, and the alloy raw material is cooled to between 20-30℃ between 95-110 seconds.

2. The method for repairing phosphorus segregation of a substrate for producing an OLED metal mask according to claim 1, characterized in that: In the low tension high temperature annealing stage, the low tension is set to 100N.

3. The method for repairing phosphorus segregation of a substrate for producing an OLED metal mask according to claim 2, characterized in that: The preheating time was set at 90 seconds and the preheating temperature was set at 300°C.

4. The method for repairing phosphorus segregation of a substrate for producing an OLED metal mask according to claim 3, characterized in that: The heating temperature was set to 900°C, the heating time was set to 600 seconds, and the holding time was set to 800 seconds.

5. The method for repairing phosphorus segregation of a substrate for producing an OLED metal mask according to claim 4, characterized in that: In the low tension high temperature annealing cooling stage, the furnace temperature was set to 25 °C, combined with inert gas for rapid cooling within 100 seconds.

6. The method for repairing phosphorus segregation of a substrate for producing an OLED metal mask according to claim 1, characterized in that: In the high tension low temperature annealing stage, the high tension is set to 200N.

7. The method for repairing phosphorus segregation of a substrate for producing an OLED metal mask according to claim 6, characterized in that: The preheating time was set to 90 seconds and the preheating temperature was set to 200°C.

8. The method for repairing phosphorus segregation of a substrate for producing an OLED metal mask according to claim 7, characterized in that: The heating temperature was set to 500°C and the heating time was set to 600 seconds.

9. The method for repairing phosphorus segregation of a substrate for producing an OLED metal mask according to claim 8, characterized in that: The holding time was set to 500 seconds.

10. The method for repairing phosphorus segregation of a substrate for producing an OLED metal mask according to claim 9, characterized in that: In the high-tension low-temperature annealing cooling stage, the furnace temperature was set to 25 °C, combined with inert gas for rapid cooling within 100 seconds.

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